Rapid determination of hexabromocyclododecane enantiomers in animal meat by matrix solid phase dispersion coupled with LC-MS/MS.

A rapid and sensitive method was developed based on matrix solid phase dispersion (MSPD) for the determination of hexabromocyclododecane enantiomers (±α, ±ß and ± Î³-HBCD) in animal meat. The instrumental analysis was employed with liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) at trace level (ng g-1). To obtain excellent efficiency, the key parameters, including the type of dispersive adsorbent and elution solvent, were investigated by single-factor experiments. The volume of elution solvent and amount of dispersive adsorbent were optimized by the Box-Behnken design through response surface methodology. Under optimized conditions, the developed method exhibited excellent methodologic characteristics and was applied to the determination of HBCD enantiomers in real chicken and pork meat. Experimental results indicated that the proposed method would be an efficient, rapid and application method for the determination of lipophilic organic pollutants in animal meat.

Carbon nanotube composite microspheres as a highly efficient solid-phase microextraction coating for sensitive determination of phthalate acid esters in water samples.

Multiwalled carbon nanotubes (MWCNTs) on polystyrene (PS) microspheres have been designed and prepared by layer-by-layer assembly via electrostatic interaction. MWCNTs@PS was characterized by scanning electron microscopy (SEM) and thermogravimetric analysis (TGA). The new materials were employed as a novel solid-phase microextraction (SPME) coating to enrich trace level of phthalate acid esters (PAEs) in water samples. Five PAEs, di-n-butyl phthalate (DBP), benzyl butyl phthalate (BBP), di-2-ethylhexyl adipate (DEHA), di-2-ethylhexyl phthalate (DEHP) and di-n-octyl phthalate (DOP), were studied in this work. The Box-Behnken design was applied to calculate optimum extraction factors affecting the extraction efficiency using a response surface. In the optimized conditions, the developed technique achieved high enrichment factors (738-2347), low limits of detection (0.0012-0.018µgL-1) and wide linearity (0.001-5µgL-1) for detecting PAEs. The method was successfully applied to analyze PAEs in real environmental water samples with recovery ranging from 73.4% to 103.8%. The results demonstrated that MWCNTs@PS are a promising coating material in the SPME of PAEs at trace levels from environmental samples.

Determination of hexabromocyclododecane enantiomers in chicken whole blood by a modified quick, easy, cheap, effective, rugged, and safe method with liquid chromatography and tandem mass spectrometry.

A rapid and simple analytical method has been developed for the determination of hexabromocyclododecane enantiomers in chicken whole blood, based on a modified quick, easy, cheap, effective, rugged, and safe approach before liquid chromatography coupled with tandem mass spectrometry. The factors influencing performance of method were investigated by single factor experiment, and further optimized by the response surface methodology based on Box-Behnken design. The matrix effects were also evaluated by the isotopic dilution method. Under the optimal conditions, the proposed method showed good linearity within the range of 1-500 µg/L and good repeatability with relative standard deviation less than 9.5% (n = 5). The limits of detection (S/N = 3) were 0.03-0.19 µg/L. The developed method was successfully applied for the analysis of hexabromocyclododecane enantiomers in real chicken blood samples. The satisfactory recoveries ranging of 83.6-115.0% were obtained (at spiked levels of 5, 20, and 100 µg/L). The results demonstrated that the proposed method would be a practical value method for the determination of hexabromocyclododecane enantiomers in animal blood. It would be further developed with confidence to analyze other lipophilic organic pollutants in blood sample.

Application of sub-Doppler DAVLL to laser frequency stabilization in atomic cesium.

We achieve laser frequency stabilization by a simple technique based on sub-Doppler dichroic atomic vapor laser lock (DAVLL) in atomic cesium. The technique that combines saturated-absorption spectroscopy and Zeeman splitting of hyperfine structures allows us to obtain a modulation-free dispersion-like error signal for frequency stabilization. For the error signal, the dependence of peak-to-peak amplitude and the slope at the zero-crossing point on the magnetic field is studied by simulation and experiment. Based on the result, we obtain an available sub-Doppler DAVLL error signal with high sensitivity to the frequency drift by selecting an appropriate strength of the magnetic field. Ultimately, the fluctuation of the locked laser frequency is confined to below 0.5 MHz in a long term, exhibiting efficient suppression of frequency noise.

Simple, reliable, and nondestructive method for the measurement of vacuum pressure without specialized equipment.

We present a simple, reliable, and nondestructive method for the measurement of vacuum pressure in a magneto-optical trap. The vacuum pressure is verified to be proportional to the collision rate constant between cold atoms and the background gas with a coefficient k, which can be calculated by means of the simple ideal gas law. The rate constant for loss due to collisions with all background gases can be derived from the total collision loss rate by a series of loading curves of cold atoms under different trapping laser intensities. The presented method is also applicable for other cold atomic systems and meets the miniaturization requirement of commercial applications.

Preconcentration and determination of polybrominated diphenyl ethers in environmental water samples by solid-phase microextraction with Fe3O4-coated bamboo charcoal fibers prior to gas chromatography-mass spectrometry.

In this paper, bamboo charcoals were modified using Fe3O4 nanosheets for the first time. The composites, as a novel solid-phase microextraction (SPME) fiber coating, were used for the extraction of seven polybrominated diphenyl ethers (PBDEs) in environmental water samples. The extraction factors (stirring rate, extraction time, and ionic strength) and desorption factors (desorption time and desorption temperature) of the fibers were systematically investigated and optimized. Under optimum conditions, the linear range was 1-1000 ng L(-1). Based on the ratio of chromatographic signal to base line noise (SN(-1)=3), the limits of detection (LODs) can reach 0.25-0.62 ng L(-1). The novel method was successful in the analysis of PBDEs in real environmental water samples. The results indicate that bamboo charcoal/Fe3O4 as an SPME coating material coupled with gas chromatography-negative chemical ionization-mass spectrometry is an excellent method for the routine analysis of PBDEs at trace levels in environmental water samples.

Rapid analysis of polybrominated diphenyl ethers in soil by matrix solid-phase dispersion using bamboo charcoal as dispersive sorbent.

An expeditious and sensitive method for the analysis of eight major polybrominated diphenyl ethers (PBDEs) in soil is presented in this study. The method is based on matrix solid-phase dispersion (MSPD) extraction and gas chromatography with negative chemical ionization mass spectrometry. Bamboo charcoal, a cheap and potentially useful material, was selected for the first time as the MSPD dispersive sorbent. Parameters affecting the extraction efficiency, including the ratio of sorbent to sample, and the type and amount of eluent, were investigated and optimized in detail. Under optimal conditions, the spiked recovery of the PBDEs was in the range 71.7-105.9%, and the limits of detection varied from 10 to 400 pg g(-1) (dry weight). Excellent linearity with correlation coefficients (r(2)) of 0.9992-0.9999 was obtained over the concentration range of 0.10-500 ng g(-1) , except for BDE-209, for which the effective concentration range was 1.0-5000 ng g(-1) . The developed method has been successfully applied to the analysis of PBDEs in real soil samples.

Preconcentration and sensitive determination of hexabromocyclododecane diastereomers in environmental water samples using solid phase extraction with bamboo charcoal cartridge prior to rapid resolution liquid chromatography-electrospray tandem mass spectrometry.

In this paper, a simple and cheap method for the simultaneous preconcentration and sensitive determination of three hexabromocyclododecane (HBCD) diastereomers (α-, ß-, and γ-HBCD) in environmental water samples has been developed. It was based on solid phase extraction (SPE) and rapid resolution liquid chromatography-electrospray tandem mass spectrometry. Bamboo charcoal, one kind of cheap material, was investigated and used as SPE adsorbent for the enrichment and determination of HBCD diastereomers. Related important parameters affecting extraction efficiencies, including type and volume of eluant, amount of sorbent, sample pH, flow rate, and sample volume, were investigated and optimized in detail. Under the optimum conditions, experimental data exhibited excellent linear relationships between peak area and concentrations over the range 0.1-10 µg L(-1). The limits of detection and precision were in the range of 0.005-0.015 µg L(-1) and 4.59-7.47%, respectively. The proposed method has been successfully applied for the trace analysis of HBCD diastereomers in real-world environmental water samples.

Temperature-controlled ionic liquid dispersive liquid-phase microextraction for the sensitive determination of triclosan and triclocarban in environmental water samples prior to HPLC-ESI-MS/MS.

A novel dispersive liquid-phase microextraction method without dispersive solvents has been developed for the enrichment and sensitive determination of triclosan and triclocarban in environmental water samples prior to HPLC-ESI-MS/MS. This method used only green solvent 1-hexyl-3-methylimidazolium hexafluorophosphate as extraction solvent and overcame the demerits of the use of toxic solvents and the instability of the suspending drop in single drop liquid-phase microextraction. Important factors that may influence the enrichment efficiencies, such as volume of ionic liquid, pH of solutions, extraction time, centrifuging time and temperature, were systematically investigated and optimized. Under optimum conditions, linearity of the method was observed in the range of 0.1-20 microg/L for triclocarban and 0.5-100 microg/L for triclosan, respectively, with adequate correlation coefficients (R>0.9990). The proposed method has been found to have excellent detection sensitivity with LODs of 0.04 and 0.3 microg/L, and precisions of 4.7 and 6.0% (RSDs, n=5) for triclocarban and triclosan, respectively. This method has been successfully applied to analyze real water samples and satisfactory results were achieved.

Highly sensitive determination of tetrabromobisphenol A and bisphenol A in environmental water samples by solid-phase extraction and liquid chromatography-tandem mass spectrometry.

Using bamboo-activated charcoal as SPE adsorbent, a novel SPE method was developed for the sensitive determination of tetrabromobisphenol A and bisphenol A in environmental water samples by rapid-resolution LC-ESI-MS/MS. Important parameters influencing extraction efficiency, including type of eluent, eluent volume, sample pH, volume and flow rate, were investigated and optimized. Under the optimal extraction conditions (eluent: 8 mL methanol, pH: 7; flow rate: 4 mL/min; sample volume: 100 mL), low LODs (0.01-0.02 ng/mL), good repeatability (6.2-8.3%) and wide linearity range (0.10-10 ng/mL) were obtained. Satisfied results were achieved when the proposed method was applied to determine the two target compounds in real-world environmental water samples with spiked recoveries over the range of 80.5-119.8%. All these facts indicate that trace determination of tetrabromobisphenol A and bisphenol A in real-world environmental water samples can be realized by bamboo-activated charcoal SPE-rapid resolution-LC-ESI-MS/MS.

Trace determination of triclosan and triclocarban in environmental water samples with ionic liquid dispersive liquid-phase microextraction prior to HPLC-ESI-MS-MS.

A novel and environmentally friendly microextraction method, termed ionic liquid dispersive liquid-phase microextraction (IL-DLPME), has been developed for rapid enrichment of triclosan and triclocarban before analysis by high-performance liquid phase chromatography-electrospray tandem mass spectrometry (HPLC-ESI-MS-MS). Instead of using toxic organic solvents, an ionic liquid was used as a green extraction solvent. This also avoided the instability of the suspending drop in single-drop liquid-phase microextraction, and the heating and cooling step in temperature-controlled ionic liquid dispersive liquid phase microextraction. Factors that may affect the enrichment efficiency, for example volume of ionic liquid, type and volume of dispersive solvent, pH, extraction time, and NaCl content were investigated in detail and optimized. Under optimum conditions, linearity of the method was observed over the range 0.2-12 microg L(-1) for triclocarban and 1-60 microg L(-1) for triclosan with correlation coefficients ranging from 0.9980 to 0.9990, respectively. The sensitivity of the proposed method was found to be excellent, with limits of detection in the range 0.040-0.58 microg L(-1) and precision in the range 7.0-8.8% (RSD, n = 5). This method has been successfully used to analyze real environmental water samples and satisfactory results were achieved. Average recoveries of spiked compounds were in the range 70.0-103.5%. All these results indicated that the developed method would be a green method for rapid determination of triclosan and triclocarban at trace levels in environmental water samples.

Sensitive determination of phenols in environmental water samples with SPE packed with bamboo carbon prior to HPLC.

Bamboo carbon, an inexpensive, readily available material, has attracted great attention in recent years because of adsorptive properties. In this paper, the potential of bamboo carbon as a SPE adsorbent for the determination of phenols, was investigated. Phenols are important environmental contaminants that may adversely affect human health. Parameters influencing extraction efficiency, including type of eluent, eluent volume, amount of adsorbent, as well as sample pH, volume, and flow rate were investigated and optimized. The optimized results exhibited excellent linear relationships between peak area and phenol concentrations over the range of 2.0-100 ng/mL, with precision between 2.2-7.2%. The LODs were 0.06-0.4 ng/mL for the eight phenols tested. The proposed method has been successfully applied to the analysis of several real-world environmental water samples. These results indicate that bamboo carbon may be used as a novel SPE adsorbent for the concentration and determination of phenols in real environmental water samples.

Rapid determination of amide herbicides in environmental water samples with dispersive liquid-liquid microextraction prior to gas chromatography-mass spectrometry.

This paper describes a novel, simple and environmentally friendly method for rapid determination of the amide herbicides metoalchlor, acetochlor, and butachlor. It is based on dispersive liquid-liquid microextraction and gas chromatography-mass spectrometry. Factors that may influence the enrichment efficiency, such as type and volume of extraction solvent, type and volume of dispersive solvent, extraction time, and content of NaCl, were investigated and optimized in detail. Under the optimum conditions, the limits of detection of metoalchlor, acetochlor, and butachlor were 0.02, 0.04, and 0.003 microg L(-1), respectively. The experimental results indicated that there was linearity over the range 0.1-50 microg L(-1) and good reproducibility with relative standard deviations over the range 1.6-3.0% (n = 5). The proposed method has been applied for the analysis of real-world water samples, and satisfactory results were achieved. Average recoveries of spiked herbicides were in the range 80.3-108.8%. All of these indicated that the developed method would be an efficient method for simultaneous determination of the three herbicides in environmental water samples.

Application of bamboo charcoal as solid-phase extraction adsorbent for the determination of atrazine and simazine in environmental water samples by high-performance liquid chromatography-ultraviolet detector.

In this article, a new method for the determination of triazine herbicides atrazine and simazine in environment aqueous samples was developed. It was based on solid-phase extraction (SPE) using bamboo charcoal as adsorbent and high-performance liquid chromatography-ultraviolet detector (HPLC-UV) for the enrichment and determination of atrazine and simazine at trace level. Related important factors influencing the extraction efficiency, such as the kind of eluent and its volume, flow rate of the sample, pH of the sample, and volume of the sample, were investigated and optimized in detail. Under the optimal conditions, the experimental results showed that excellent linearity was obtained over the range of 0.5-30 microg L(-1) with correlation coefficients 0.9991 and 0.9982, for atrazine and simazine, respectively; and the relative standard deviations of two analytes were 8.3, 8.7%, respectively. The proposed method was successfully applied to the analysis of tap water and well water samples. And satisfactory spiked recoveries were obtained in the range of 75.2-107.1%. The above results indicated that the developed method was an excellent alternative for the routine analysis in environmental field.

Using bamboo charcoal as solid-phase extraction adsorbent for the ultratrace-level determination of perfluorooctanoic acid in water samples by high-performance liquid chromatography-mass spectrometry.

In recent years, bamboo charcoal, a new kind of material with special microporous and biological characteristics, has attracted great attention in many application fields. In this paper, the potential of bamboo charcoal to act as a solid-phase extraction (SPE) adsorbent for the enrichment of the environmental pollutant perfluorooctanoic acid, which is one of the newest types of persistent organic pollutants in the environment, has been investigated. Important factors that may influence the enrichment efficiency--such as the eluent and its volume, the flow rate of the sample, the pH of the sample and the sample volume--were investigated and optimized in detail. Under the optimum conditions, the limit of detection for PFOA was 0.2 ng L(-1). The experimental results indicated that this approach gives good linearity (R(2) = 0.9995) over the range 1-1000 ng L(-1) and good reproducibility, with a relative standard deviation of 4.0% (n = 5). The proposed method has been applied to the analysis of real water samples, and satisfactory results were obtained. The average spiked recoveries were in the range 79.5-118.3%. All of the results indicate that the proposed method could be used for the determination of PFOA at ultratrace levels in water samples.

Investigation of feasibility of bamboo charcoal as solid-phase extraction adsorbent for the enrichment and determination of four phthalate esters in environmental water samples.

This paper demonstrates, for the first time, that adsorptive potential of bamboo charcoal for solid-phase extraction of phthalate esters was investigated. The four phthalate esters, dimethyl phthalate (DMP), diethyl phthalate (DEP), butyl benzyl phthalate (BBP) and di-n-butyl phthalate (DBP), are quantitatively adsorbed on a bamboo charcoal packed cartridge, then the analytes retained on the cartridge are quantitatively desorbed with optimum amounts of acetone. Finally, the analytes in the eluant acetone are determined by high-performance liquid chromatography-ultraviolet detectior. Important parameters influencing the extraction efficiency, such as eluant and its volume, flow rate of sample, sample volume, pH, the amount of adsorbent and ionic strength were investigated and optimized in detail. Under the optimum conditions, the limits of detection were 0.35-0.43 microg/L for four phthalate esters. The proposed method has been applied to the analysis of rainwater and tap water samples. And satisfactory spiked recoveries were obtained in the range of 75.0-114.2%. All the results indicated that the bamboo charcoal has great potential as a novel adsorbent material for the enrichment and determination of phthalate esters in real environmental water samples.

Nonequilibrium hollow-fiber liquid-phase microextraction with in situ derivatization for the measurement of triclosan in aqueous samples by gas chromatography-mass spectrometry.

Hollow-fiber liquid-phase microextraction (HF-LPME), a relatively new sample preparation technique, has attracted much interest in the field of environmental analysis. In the current study, a novel method based on hollow-fiber liquid-phase microextraction with in situ derivatization and gas chromatography-mass spectrometry for the measurement of triclosan in aqueous samples is described. Hollow-fiber liquid-phase microextraction conditions such as the type of extraction solvent, the stirring rate, the volume of derivatizing reagent, and the extraction time were investigated. When the conditions had been optimized, the linear range was found to be 0.05-100 microg l(-1) for triclosan, and the limit of detection to be 0.02 microg l(-1). Tap water and surface water samples collected from our laboratory and Wohushan reservoir, respectively, were successfully analyzed using the proposed method. The recoveries from the spiked water samples were 83.6 and 114.1%, respectively; and the relative standard deviation (RSD) at the 1.0 microg l(-1) level was 6.9%.

Sensitive measurement of ultratrace phenols in natural water by purge-and-trap with in situ acetylation coupled with gas chromatography-mass spectrometry.

A novel purge-and-trap method coupled with gas chromatography-mass spectrometry (GC-MS) is developed for the analysis of trace and ultratrace phenols based on their derivatization with acetic anhydride. Parameters affecting the extraction efficiency, such as purge temperature, concentration of sodium chloride, purge time, and volume of derivatization reagent, were investigated. The optimized conditions were addition of 150 microL acetic anhydride, purge time of 25 min at the purge temperature of 60 degrees C with 30% NaCl. The linear range was 0.2-100 microg L(-1) for phenols. The limits of detection (LODs) ranged from 0.08 to 0.15 microg L(-1) and the relative standard deviations (RSDs) for most of the phenols at the 10 microg L(-1) level were below 10%. Natural water samples collected from a pool were successfully analyzed using the proposed method. The recovery of spiked water samples was 72.9-84.2%.

Application of liquid-phase microextraction and gas chromatography-mass spectrometry for the determination of chloroform in drinking water.

In this paper, a novel method for the determination of chloroform in drinking water has been described. It is based on liquid-phase microextraction (LPME) and gas chromatography-mass spectrometry (GC-MS). Extraction conditions such as solvent selection, organic solvent dropsize, stirring rate, content of NaCl and extraction time were found to have significant influence on extraction efficiency. The optimized conditions were 1.5 microl xylene, 20 min extraction time at 400 rpm stirring rate without NaCl addition. The linear range was 1.0 - 100 microg l(-1) for chloroform. The limit of detection (LOD) was 1.0 microg l(-1); and relative standard deviation (RSD) at the 30 microg l(-1) level was 2.9%. Tap water samples from a laboratory were successfully analyzed using the proposed method. The relative recovery of spiked water samples was 104%.